CN110828819B - Pyrrhotite type iron sulfide negative electrode material for potassium ion battery and preparation method thereof - Google Patents
Pyrrhotite type iron sulfide negative electrode material for potassium ion battery and preparation method thereof Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
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Abstract
A pyrrhotite type iron sulfide negative electrode material for a potassium ion battery and a preparation method thereof belong to the field of potassium ion batteries. The method comprises the following specific steps: dissolving ferric nitrate nonahydrate and polyvinylpyrrolidone in deionized water to prepare a mixed solution, drying the mixed solution, grinding the dried mixed solution into powder, and placing the powder in a tubular furnace to heat and preserve heat in a hydrogen-argon mixed atmosphere to obtain the iron nanoparticle modified three-dimensional graphene; and then, placing the three-dimensional graphene modified by the iron nanoparticles in an air atmosphere for heat treatment to obtain the foamed iron oxide. Grinding and uniformly mixing the foamed iron oxide and the sublimed sulfur, then placing the mixture into a tubular furnace to heat and preserve heat in an argon atmosphere, and collecting powder products to obtain the foamed pyrrhotite type iron sulfide negative electrode material. The invention has short production period, low cost and strong repeatability, can be prepared in a large scale, shows excellent performance when used as a potassium ion battery cathode and has wide application prospect.
Description
Technical Field
The invention belongs to the field of potassium ion batteries, and particularly relates to a pyrrhotite type iron sulfide negative electrode material for a potassium ion battery and a preparation method thereof.
Background
With the continuous development of economy and the continuous progress of science and technology, the demand of energy sources is gradually increased. However, the development and utilization of traditional fossil energy sources such as coal, oil, natural gas and the like have three outstanding problems: resource exhaustion, climate warming and environmental pollution. The development of renewable energy sources such as solar energy, wind energy, tidal energy and the like is a necessary trend for solving the outstanding problems of non-renewable energy sources and ensuring the sustainable development of human beings. However, these renewable energy sources are highly dependent on weather and climate, and have volatility and randomness, so that it is urgently needed to develop large-scale energy storage technology to make the renewable energy sources cooperate with the power grid to stably operate. In current energy storage devices, lithium ion batteries are applied to the fields of portable electronic devices, electric vehicles and the like on a large scale due to high energy density, but the rising price and extremely low storage capacity of lithium resources limit their application to large-scale stationary power storage. Therefore, there is a need to develop a new rechargeable battery with low cost, abundant natural resources, long life, high energy density and power density, which is used as a substitute for lithium ion battery for portable electronic devices, electric vehicles and smart grids in the future.
In recent years, a novel secondary battery such as a potassium ion or sodium ion has been drawing attention from researchers because of its electrochemical principle similar to that of a lithium ion battery. The potassium ion battery has the advantages of rich resources and low cost, and the K/K + has the standard oxidation-reduction potential closest to Li/Li +, so that the potassium ion battery can present high energy density. At present, a great amount of Carbon materials are reported to be used as negative electrode materials of potassium ion batteries (137 (2015)11566-11569), but the theoretical specific capacity of the Carbon materials is low, and the requirement of high energy density cannot be met. Therefore, the development of the high-capacity cathode material capable of keeping stable structure in the potassium ion de-intercalation process has very important practical significance.
Disclosure of Invention
The invention aims to provide a pyrrhotite type iron sulfide negative electrode material for a potassium ion battery and a preparation method, which are simple, efficient, low in cost and capable of being used for preparing the potassium ion battery in a large scale.
In order to achieve the purpose, the invention adopts the technical scheme that:
a pyrrhotite type iron sulfide negative electrode material for a potassium ion battery has a chemical formula of FexS is anda conductor phase having excellent conductivity, wherein x is 0.5. ltoreq. x.ltoreq.1; the cathode material is of a layered structure, potassium ions can be stored among layers, and after the potassium ions are firstly de-intercalated, the structure is converted into K with larger interlayer spacingyFexS is favorable for the subsequent potassium extraction process, wherein y is more than or equal to 0 and less than or equal to 0.5.
The preparation method of the pyrrhotite type iron sulfide negative electrode material for the potassium ion battery comprises the following steps:
a. dissolving ferric nitrate nonahydrate and polyvinylpyrrolidone (K30) in deionized water, ultrasonically stirring for 8-12min to obtain a mixed solution, completely drying, and grinding into powder;
b. transferring the ground powder into a crucible, then placing the crucible into a tubular furnace, heating to 900-950 ℃ at a heating rate of 5-10 ℃/min in a hydrogen-argon mixed gas atmosphere, preserving heat for 1-2 h, and collecting a black foam product after the tubular furnace is cooled to room temperature, namely the iron nanoparticle modified three-dimensional graphene composite material;
c. carrying out heat treatment on the obtained iron nanoparticle modified three-dimensional graphene composite material in an air atmosphere to obtain a red foam-like product, namely the foam iron oxide;
d. grinding and mixing the foamed iron oxide and the sublimed sulfur, then heating to 500-600 ℃ at a heating rate of 2-5 ℃/min in an argon mixed gas atmosphere, preserving heat for 2-3 h, and collecting a foamed product after the tubular furnace is cooled to room temperature, namely the pyrrhotite type foamed iron sulfide.
Further, the mass ratio of the ferric nitrate nonahydrate to the polyvinylpyrrolidone (K30) in the step a is (1.5-1.8): 1.
further, in the hydrogen-argon mixed gas in the step b, the volume content of argon is 70-90%, and the volume content of hydrogen is 10-30%.
Further, the heat treatment temperature in the step c is 350-400 ℃, and the heat preservation time is 3-4 hours.
Further, the mass ratio of the foamed iron oxide to the sublimed sulfur in the step d is 1: (2.0-3.0).
Compared with the prior art, the invention has the beneficial effects that:
1) the chemical formula of the cathode material is FexS is a conductor phase and has excellent conductivity, wherein x is more than or equal to 0.5 and less than or equal to 1; the cathode material is of a layered structure, potassium ions can be stored among layers, and after the potassium ions are firstly de-intercalated, the structure is converted into K with larger interlayer spacingyFexS is favorable for the subsequent potassium extraction process, wherein y is more than or equal to 0 and less than or equal to 0.5.
2) By accurately controlling the reactant content and the temperature, the pyrrhotite type foamed iron sulfide with different components and different appearances can be prepared in a shorter time.
3) The method is simple and easy to operate, has low cost and can be used for large-scale preparation.
Drawings
Fig. 1 is a FESEM photograph of a pyrrhotite-type foamed iron sulfide prepared in accordance with the present invention.
FIG. 2 is a TEM photograph of a pyrrhotite-type foamed iron sulfide prepared according to the present invention.
FIG. 3 is a graph showing the potassium storage performance of a pyrrhotite type foamed iron sulfide prepared in accordance with the present invention
Detailed Description
Example one
Weighing polyvinylpyrrolidone (K30) and ferric nitrate nonahydrate according to a mass ratio of 1:1.5, dissolving the ferric nitrate nonahydrate and the polyvinylpyrrolidone in deionized water, ultrasonically stirring for 10min to prepare a mixed solution, then placing the mixed solution in a drying oven, keeping the temperature at 80 ℃ until the mixed solution is completely dried, grinding the mixed solution into powder, transferring the powder into a crucible, placing the crucible in a tubular furnace, heating the crucible to 900 ℃ at a heating rate of 5 ℃/min in an atmosphere of hydrogen-argon mixed gas (the volume ratio of hydrogen to argon is 1:9), keeping the temperature for 2h, cooling the tubular furnace, and collecting black foam products to obtain the iron nanoparticle modified three-dimensional graphene composite material. Then carrying out heat treatment on the obtained three-dimensional graphene composite material modified by the iron nanoparticles for 3h at 350 ℃ in the air atmosphere to obtain red foamy iron oxide; and then weighing the foamed iron oxide and the sublimed sulfur according to the mass ratio of 1:2, grinding and uniformly mixing, placing in a tubular furnace, heating to 550 ℃ at the heating rate of 4 ℃/min in the argon atmosphere, preserving heat for 2 hours, and collecting a foamed product after the tubular furnace is cooled, namely the pyrrhotite type foamed iron sulfide. See figures 1 and 2 for specific data.
The electrochemical test method of the pyrrhotite type foam iron sulfide negative electrode material comprises the following steps:
mixing pyrrhotite type foam iron sulfide negative electrode material, conductive agent Keqin black and binder polyvinylidene fluoride (PVDF) according to the mass ratio of 8:1:1, grinding uniformly, adding a proper amount of N-methyl pyrrolidone (NMP) to prepare slurry, and uniformly coating the slurry on a copper foil. Vacuum drying at 100 deg.C for 10 hr, and cutting into electrode plate with diameter of 10mm with a slicer. 1mol/LKPF with metal potassium sheet as counter electrode and glass fiber as diaphragm6the/DGM is electrolyte and is assembled into a CR2032 button cell in an argon protective glove box. And standing for 12 hours after the battery is assembled, and performing constant-current charge and discharge test by using a LAND CT2001A battery test system, wherein the test voltage is 0.5-3.0V, and the current density is 200 mA/g. See figure 3 for specific data.
Example two
Weighing polyvinylpyrrolidone (K30) and ferric nitrate nonahydrate according to a mass ratio of 1:1.8, dissolving the ferric nitrate nonahydrate and the polyvinylpyrrolidone in deionized water, ultrasonically stirring for 10min to prepare a mixed solution, then placing the mixed solution in a drying oven, keeping the temperature at 80 ℃ until the mixed solution is completely dried, grinding the mixed solution into powder, transferring the powder into a crucible, placing the crucible in a tubular furnace, heating the crucible to 900 ℃ at a heating rate of 5 ℃/min in an atmosphere of hydrogen-argon mixed gas (the volume ratio of hydrogen to argon is 1:9), keeping the temperature for 2h, cooling the tubular furnace, and collecting black foam products to obtain the iron nanoparticle modified three-dimensional graphene composite material. Then carrying out heat treatment on the obtained three-dimensional graphene composite material modified by the iron nanoparticles for 3h at 350 ℃ in the air atmosphere to obtain red foamy iron oxide; and then weighing the foamed iron oxide and the sublimed sulfur according to the mass ratio of 1:2, grinding and uniformly mixing, placing in a tubular furnace, heating to 550 ℃ at the heating rate of 4 ℃/min in the argon atmosphere, preserving heat for 2 hours, and collecting a foamed product after the tubular furnace is cooled, namely the pyrrhotite type foamed iron sulfide.
EXAMPLE III
Weighing polyvinylpyrrolidone (K30) and ferric nitrate nonahydrate according to a mass ratio of 1:1.5, dissolving the ferric nitrate nonahydrate and the polyvinylpyrrolidone in deionized water, ultrasonically stirring for 10min to prepare a mixed solution, then placing the mixed solution in a drying oven, keeping the temperature at 80 ℃ until the mixed solution is completely dried, grinding the mixed solution into powder, transferring the powder into a crucible, placing the crucible in a tubular furnace, heating the crucible to 900 ℃ at a heating rate of 5 ℃/min in an atmosphere of hydrogen-argon mixed gas (the volume ratio of hydrogen to argon is 2:8), keeping the temperature for 2h, cooling the tubular furnace, and collecting black foam products to obtain the iron nanoparticle modified three-dimensional graphene composite material. Then carrying out heat treatment on the obtained three-dimensional graphene composite material modified by the iron nanoparticles for 3h at 350 ℃ in the air atmosphere to obtain red foamy iron oxide; and then weighing the foamed iron oxide and the sublimed sulfur according to the mass ratio of 1:2, grinding and uniformly mixing, placing in a tubular furnace, heating to 550 ℃ at the heating rate of 4 ℃/min in the argon atmosphere, preserving heat for 2 hours, and collecting a foamed product after the tubular furnace is cooled, namely the pyrrhotite type foamed iron sulfide.
Example four
Weighing polyvinylpyrrolidone (K30) and ferric nitrate nonahydrate according to a mass ratio of 1:1.8, dissolving the ferric nitrate nonahydrate and the polyvinylpyrrolidone in deionized water, ultrasonically stirring for 10min to prepare a mixed solution, then placing the mixed solution in a drying oven, keeping the temperature at 80 ℃ until the mixed solution is completely dried, grinding the mixed solution into powder, transferring the powder into a crucible, placing the crucible in a tubular furnace, heating the crucible to 950 ℃ in an atmosphere of hydrogen-argon mixed gas (the volume ratio of hydrogen to argon is 2:8) at a heating rate of 5 ℃/min, keeping the temperature for 2h, and collecting black foam products after the tubular furnace is cooled to obtain the iron nanoparticle modified three-dimensional graphene composite material. Then carrying out heat treatment on the obtained three-dimensional graphene composite material modified by the iron nanoparticles for 3h at 350 ℃ in the air atmosphere to obtain red foamy iron oxide; and then weighing the foamed iron oxide and the sublimed sulfur according to the mass ratio of 1:2, grinding and uniformly mixing, placing in a tubular furnace, heating to 550 ℃ at the heating rate of 4 ℃/min in the argon atmosphere, preserving heat for 2 hours, and collecting a foamed product after the tubular furnace is cooled, namely the pyrrhotite type foamed iron sulfide.
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and it should be understood by those skilled in the art that the specific embodiments of the present invention can be modified or substituted with equivalents with reference to the above embodiments, and any modifications or equivalents without departing from the spirit and scope of the present invention are within the scope of the claims to be appended.
Claims (5)
1. A preparation method of a pyrrhotite type iron sulfide negative electrode material for a potassium ion battery is characterized by comprising the following steps of:
a. dissolving ferric nitrate nonahydrate and polyvinylpyrrolidone K30 in deionized water, ultrasonically stirring for 8-12min to obtain a mixed solution, completely drying, and grinding into powder;
b. transferring the ground powder into a crucible, then placing the crucible into a tubular furnace, heating to 900-950 ℃ at a heating rate of 5-10 ℃/min in a hydrogen-argon mixed gas atmosphere, preserving heat for 1-2 h, and collecting a black foam product after the tubular furnace is cooled to room temperature, namely the iron nanoparticle modified three-dimensional graphene composite material;
c. carrying out heat treatment on the obtained iron nanoparticle modified three-dimensional graphene composite material in an air atmosphere to obtain a red foam-like product, namely the foam iron oxide;
d. grinding and mixing the foamed iron oxide and the sublimed sulfur, then heating to 500-600 ℃ at a heating rate of 2-5 ℃/min in an argon mixed gas atmosphere, preserving heat for 2-3 h, and collecting a foamed product after the tubular furnace is cooled to room temperature, namely the pyrrhotite type foamed iron sulfide;
the chemical formula of the cathode material is FexS is a conductor phase and has excellent conductivity, wherein x is more than or equal to 0.5 and less than or equal to 1; the cathode material is of a layered structure, potassium ions can be stored among layers, and after the potassium ions are firstly de-intercalated, the structure is converted into K with larger interlayer spacingyFexS is favorable for the subsequent potassium extraction process, wherein y is more than or equal to 0 and less than or equal to 0.5.
2. The method for preparing the pyrrhotite-type iron sulfide negative electrode material for the potassium ion battery according to claim 1, wherein the mass ratio of the iron nitrate nonahydrate to the polyvinylpyrrolidone K30 in the step a is (1.5-1.8): 1.
3. the method for producing a pyrrhotite-type iron sulfide negative electrode material for a potassium ion battery according to claim 1, characterized in that the hydrogen-argon mixed gas in the step b contains 70 to 90% by volume of argon and 10 to 30% by volume of hydrogen.
4. The preparation method of the pyrrhotite type iron sulfide negative electrode material for the potassium ion battery according to claim 1, wherein the heat treatment temperature in the step c is 350-400 ℃, and the heat preservation time is 3-4 hours.
5. The method for producing a pyrrhotite-type iron sulfide negative electrode material for a potassium ion battery according to claim 1, characterized in that the mass ratio of the foamed iron oxide to the sublimed sulfur in the step d is 1: (2.0-3.0).
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